Novel advanced thermoset composites with intrinsic recyclability · 2021. 7. 17. · of MRO...

© CIDETEC 2018

Novel advanced thermoset

composites with intrinsic

recyclability

Innovations in Carbon Fibres and composite materials Recycling Leitat, October 8th

Alaitz Rekondo Head of Polymers & Composites unit

Contact: [email protected]

CIDETEC is an organization for applied research that

integrates three international reference institutes in the fields

of energy storage, surface engineering and nanomedicine.

Pilot Plant for GMP manufacturing_1080p.mp4

Outline

Introduction & concepts

Epoxy vitrimers based on aromatic disulfide

Dynamic fibre reinforced thermoset composites

AIRPOXY project

Novel chemical recycling process of 3R composites

Introduction & Concepts

Vitrimers based on aromatic disulfide exchange

As a model metathesis reaction, we studied the equilibration of equimolar amounts of different aromatic disulfide mixtures by 1H-NMR.

A. Rekondo, R. Martin, A. Ruiz de Luzuriaga, G. Cabañero, H. J. Grande and I. Odriozola, Mater. Horiz., 2014, 1, 237–240


Reference network

Dynamic network

Tg (DSC)

[ºC] 127 130

Tg (DMA)

[ºC] 130 130

Td [ºC] 350 300

E´(25ºC)

[GPa] 2,5 2,6

E´(150ºC)

[MPa] 20 20

Stress

[MPa] 81 88

Strain [%] 7,3 7,1

Comparable thermal and mechanical

properties using our dynamic hardener

instead of a conventional hardener.


A. Ruiz de Luzuriaga et al., Material Horizon, 2016, 3, 241.

Characterization of the stress relaxation by DMA

• At temperatures above Tg, the dynamic epoxy

network is able to completely relax stress and flow.

• The obtained relaxation times ranged from 3 hours at

130 ºC to 20 seconds at 200 ºC.



Reparable thermoset resins Recyclable thermoset resins

The dynamic character of the epoxy network offers new challenges:

a small scratch performed on a specimen was repaired

just by applying heat a pressure with a household iron



Recyclable thermoset resins

The dynamic character of the epoxy network offers new challenges:


• A new generation of Reprocessable,

Repairable and Recyclable high-

performance fibre-reinforced

thermoset composites.

• They can be manufactured following

traditional methods but the resulting

material can be reprocessed, repaired

and recycled.

3R Composites

3R composite laminates can be heated above the Tg and re-

shaped in a few minutes applying pressure, which allows the

thermoforming of cured 3R laminates to obtain 3D geometries,

in a similar way to thermoplastic composites.

This technology enables the development of high

production rate manufacturing processes for

thermoset composites reducing the

manufacturing costs of thermoset CC parts by

over 35% vs autoclave manufacturing.

> 3R Composites:

Reprocessing,

Repairing,

Recycling

35% reducing the

manufacturing

costs.


Repair of damages

based on

resin/fibre

delaminations and

resin micro-cracks

by applying heat

and pressure to

the damaged part.

ILSS: 37,2 ± 2,81 MPa

ILSS: 38,0 ± 2,4 MPa

This technology enables to reduce the current costs

of MRO associated to the reparation or replacement

of thermoset CC parts by 50% (nowadays damaged

parts are often rejected due to the high costs and repair

times of the traditional patch techniques).

50% reducing the

current costs

of MRO.

> 3R Composites:

Reprocessing,

Repairing,

Recycling


Mechanical recycling: the cured 3R composite can be ground into

flakes or pellets which can then be reprocessed by heating 80ºC above

the Tg and pressing, obtaining a new short fibre reinforced 3R composite.

This technology enables

the valorisation of the

scraps generated during

the manufacturing of

thermoset CC offering 3

different environmental

and industrial

advantages:

> 3R Composites:

Reprocessing,

Repairing,

Recycling

REDUCTION

OF LANDFILL

WASTE.

REDUCTION

OF THE COSTS

OF WASTE

MANAGEMENT

OF SCRAPS.

MANUFACTURING

OF COST

COMPETITIVE AND

SUSTAINABLE NEW

THERMOSET CC

PARTS BASED ON

VALORISED

SCRAPS.


Chemical recycling: the 3R matrix can be completely

disrupted by the addition of a specific chemical agent

without affecting the reinforcement.

> 3R Composites:

Reprocessing,

Repairing,

Recycling


The aim of AIRPOXY is to reduce the

production and maintenance costs of

composite parts in the aeronautic sector

by introducing a novel family of thermoset

composites that preserve all the advantages

of conventional thermosets, while showing

new unprecedented features such

as Re-processability, Reparability and

Recyclability (3R – Composites).

ThermoformAble, repaIrable and bondable smaRt ePOXY

based composites for aero structures

Our role.

CIDETEC acts as coordinator of the AIRPOXY project. Apart

from this role, CIDETEC is in charge of several key technical

tasks and activities, including:

- Formulation of 3R resins for aerospace composites.

- Formulation of 3R adhesives for aerospace applications.

- Fabrication and characterization of 3R aerospace

composites.

- Development of the 3R adhesive bonding process.

- Support the industrial partners regarding 3R technology.

ThermoformAble, repaIrable and bondable smaRt ePOXY

based composites for aero structures

> 3R Composites:

Reprocessing,

Repairing,

Recycling


Chemical recycling process

3R composite Composite recycling 3R resin solution Recovered fabric

> 3R Composites:

Reprocessing,

Repairing,

Recycling Recovered fabric

after 4h

Recovered fabric

after 8h

Resin

FE-SEM analysis of the recovered fabric


> 3R Composites:

Reprocessing,

Repairing,

Recycling

Recovered 3R resin

p06-0-1

Exo Down

Midpoint type: Half height Midpoint: 115,135 °C

Resina virgen

Tg= 115 ºC

D1R2 e

Exo Down

Midpoint type: Half height Midpoint: 109,317 °C

Resina recuperada

Tg= 109 ºC

Virgin 3R resin Recovered 3R resin


Thank you for your attention!

Novel advanced thermoset composites with intrinsic recyclability · 2021. 7. 17. · of MRO...

Documents

Transcript of Novel advanced thermoset composites with intrinsic recyclability · 2021. 7. 17. · of MRO...